CN105755302A - High-performance hydrogen-storage alloy and preparation method thereof - Google Patents
High-performance hydrogen-storage alloy and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a high-performance hydrogen-storage alloy and a preparation method thereof, the high-performance hydrogen-storage alloy Pd @ Mg-Y is obtained by coating Pd with Mg100-xYx (x = 20-25) alloy particles, the particles size of the alloy particle is 50 to 150 microns, and Pd film thickness is 5-30nm. The preparation method is as follows: a Mg100-xYx (x = 20-25) master alloy ingot is prepared by vacuum melting method, hydrogen storage alloy inner-core particles with a particle size of 50 to 150 microns are obtained by mechanical crushing, and the surface of the Mg100-xYx (x = 20-25) inner-core particles is uniformly coat-plated with a Pd film by magnetron sputtering coating technology. Experimental results show that: hydrogen absorption and desorption rates of the hydrogen-storage alloy Pd @ Mg-Y obtained by the method are significantly faster than the hydrogen absorption and desorption rates of pure Mg of same size, so that the large particle size Pd @ Mg77Y23 hydrogen storage alloy has a good use prospect in hydrogen storage materials, as well as simplification of the preparation process.
Description
Technical field
The present invention relates to a kind of material and preparation method thereof, in particular to a kind of hydrogen bearing alloy and preparation method thereof.
Background technology
As the hydrogen of green energy resource, due to its cleaning, have again and be easy to store and resourceful feature, so occupying critical role in following sustainable energy.So far, hindering " hydrogen economy " key factor of developing is the storage of hydrogen, and therefore the research and development of hydrogen storage material become one of hydrogen utilization key link moving towards practical and scale.Nickel-hydrogen battery negative pole material as largest application areas, it is desirable to the discharge performance that hydrogen bearing alloy has had, long cycle life, suitable hydrogen decomposition pressure etc..Magnesium-base hydrogen storage material, due to light weight, rich reserves, low price and hydrogen storage capability big (2200mAh/g), becomes one of most potential hydrogen storage material, has attracted the sight of countries in the world scientists.
But the hydrogen storage property of Mg base hydrogenous alloy is largely determined by the impact of granularity, granule is more little, inhales hydrogen desorption kinetics performance more excellent.Because: the oxygen in air is had high reaction activity by Mg, when inhaling hydrogen, can form the MgH of densification at particle surface2Hydride coatings, and MgH2Stability is high, at 0.1MPaH2Decomposition temperature under pressure reaches 300 DEG C, and hydrogen discharge reaction speed is slow, so hindering the further diffusion of hydrogen, hydrogen desorption kinetics degradation.According to bibliographical information, when hydride coatings thickness is more than 30～50 μm, hydrogen can not continue diffusion, and absorbance is close to 0.Therefore the granularity of current studied Mg base hydrogen bearing alloy is typically smaller than 60 μm.And the large scale of alloy is more suitable for industrialized production.Therefore, the performance improving bulky grain granularity hydrogen bearing alloy directly affects the industrial applications of Mg base hydrogen bearing alloy.
For the improvement problem of bulky grain hydrogen bearing alloy dynamic performance, surface modification is one of more effective method.Lid layer catalyst is covered, it is possible to promote dissociating and adsorbing of hydrogen, and then improve suction hydrogen desorption kinetics performance, Mg can also be protected to exempt from oxidation simultaneously at alloy surface.This technological approaches has shown fabulous improvement effect in Mg base film.And on bulky grain hydrogen bearing alloy, realize cladding seldom report.So needing to provide a kind of Mg base hydrogenous alloy selecting which kind of element and composition the technical scheme by which kind of cladding to obtain and have good dynamic performance.
Summary of the invention:
It is an object of the invention to provide a kind of high-performance hydrogen bearing alloy PdMg-Y.
It is a further object of the present invention to provide a kind of method preparing PdMg-Y hydrogen bearing alloy.
It is an object of the invention to the realization of following technical scheme:
High-performance hydrogen bearing alloy PdMg-Y provided by the invention, this alloy core composition is Mg100-xYxAlloying pellet, x is 20～25, and outer surface is coated with the Pd film of uniform thickness.
In first optimal technical scheme of described alloy provided by the invention, the granularity of kernel Mg-Y is 50～150 microns.
In second optimal technical scheme of described alloy provided by the invention, Pd film thickness is 5～30nm.
The preparation method of hydrogen bearing alloy PdMg-Y provided by the present invention comprises the steps:
A, dispensing: metal Mg and metal Y is according to the ratio dispensing that mol ratio is 3:1～4:1；
B, prepare foundry alloy: be placed in the graphite crucible of smelting furnace by raw material, evacuation, purges 3～5 times furnace chamber with argon, then heats the Mg being uniformly mixed and y alloy fused solution, described melting charge is poured in copper cold-crucible and condense, obtain as cast condition Mg-Y master alloy ingot；
C, the Mg-Y master alloy ingot made by step b are pulverized, and cross 100～300 mesh sieve choosings, make the alloying pellet that granularity is 50～150 microns；
D, the negative electrode being magnetron sputtering coater with Pd target, vibrate the step c alloying pellet prepared in ware at the sample of magnetron sputtering coater, be coated with Pd film, obtain hydrogen bearing alloy PdMg-Y.
In first optimal technical scheme of described alloy preparation method, the purity of metal Mg and metal Y is all more than 99.5%.
In second optimal technical scheme of described alloy preparation method, the vacuum of described b step is higher than 5 × 10-4Pa；Purity of argon >=99.999% of purging furnace chamber；After preheating 20～30 seconds, electric current is adjusted to 120～160A, after making the fusing of alloy block, electric current is risen to 200～350A again, heat 2～3 minutes.
In 3rd optimal technical scheme of described alloy preparation method, step c completes in vacuum glove box.
In 4th optimal technical scheme of described alloy preparation method, the target diameter of negative electrode Pd described in step d is 60～80mm, purity >=99.9%；Background vacuum 1 × 10-3～2 × 10-3Pa, with purity >=99.99% sputtering argon, is 40～80sccm in argon flow amount, and pressure is under 0.5～0.8Pa, and sputtering power is under 120～200W, sputters 120～300 seconds；Sample vibration ware frequency of vibration is 5～20Hz.
With immediate prior art ratio, technical scheme provided by the invention has following excellent effect:
1) adopt PdMg-Y hydrogen bearing alloy prepared by the inventive method, compared with sample prepared by traditional method, there is the advantages such as product properties index regulation and control big, quality controllable, the superior performance of degree of freedom；
2) the PdMg-Y hydrogen bearing alloy that prepared by the inventive method has kernel composition, particle diameter and the clad Pd film thickness feature such as controlled flexibly, and preparation process energy-conserving and environment-protective are pollution-free, therefore extremely suitable industrial applications.
3) PdMg-Y hydrogen bearing alloy provided by the invention is in activation process, PdMg77Y23The hydrogen-absorbing ability of granule is better than Mg77Y23Granule, hydrogen-absorption speed is significantly faster than that Mg77Y23Granule.And subsequently put in hydrogen process, hydrogen discharging rate is also significantly faster than Mg77Y23Granule.Show the Mg with sputter coating layer Pd77Y23The dynamic performance of granule is greatly improved.
Accompanying drawing explanation
Fig. 1 is vibrating device schematic diagram provided by the invention.
Fig. 2 is the PdMg of the embodiment of the present invention 1 preparation77Y23SEM pattern (a) of granule and Surface scan EDS (b) and Pd (c), Mg (d), Y (e) power spectrum mapping.
Fig. 3 is the PdMg of the embodiment of the present invention 1 preparation77Y23Granule and Mg77Y23The suction Hydrogen desorption isotherms of granule compares.
Detailed description of the invention
Embodiment 1
Prepare grain graininess 60～80 μm, cladding Pd film thickness 5nm, composition PdMg77Y23Hydrogen bearing alloy
1) dispensing
By purity all metal Mg more than 99.5% and metal Y by design composition Mg77Y23Carry out dispensing, and consider certain scaling loss (scaling loss of Y is set to 5wt%, Mg scaling loss 15wt%)；
2) alloy melting
Fine vacuum high-frequency induction smelting furnace is adopted to prepare Mg-Y foundry alloy.By step 1) raw material for preparing is placed in the graphite crucible of fine vacuum high-frequency induction smelting furnace, is evacuated to background vacuum higher than 5 × 10-4Pa, carries out 3 prepurgings then through with purity >=99.999% argon to furnace chamber, then begins to warm up: first power-on preheated crucible, after 20 seconds, adjusts electric current to 120A, makes alloy block be completely melt；Then improve melting electric current to 240A, keep 2 minutes, after Mg and y alloy fused solution at high temperature mix homogeneously, liquation is poured in copper cold-crucible and condense, obtain certain ingredients as cast condition Mg-Y mother's ingot.
3) break process
By through step 2) the Mg-Y master alloy ingot made carries out Mechanical Crushing and becomes fritter, then be placed in agate mortar and grind to form fine powder, select through 200 mesh sieves, make the alloying pellet that granularity is 60～80 microns.For avoiding granule to aoxidize in atmosphere, break process process completes in vacuum glove box.
4) magnetron sputtering Pd film
Choose diameter 60mm, purity >=99.9% Pd target as the negative electrode of magnetron sputtering coater.By through step 3) the kernel alloying pellet made be placed in magnetron sputtering coater sample vibration ware in.Sample vibration ware schematic diagram is as shown in Figure 1.
Arranging sputter coating parameter is: background vacuum 1 × 10-3Pa, adopts purity >=99.99% argon as sputter gas, and argon flow amount is 50sccm, and operating pressure is 0.6Pa, and sputtering power is 150W, and the sputter coating time is 180 seconds.Coating process sample vibration ware frequency of vibration is 5Hz, makes Pd film cladding Mg77Y23Alloying pellet, i.e. PdMg77Y23Hydrogen bearing alloy.
EDAX results shows, PdMg prepared by above-mentioned steps77Y23Hydrogen bearing alloy kernel composition is than for Mg76.8Y23.2, illustrate that female ingot composition is essentially identical with design proportioning；Observe in conjunction with granule transverse section microscopic appearance, it is known that Pd film thickness is about 5nm, meets designing requirement.
Fig. 3 is PdMg77Y23Alloy first time 350 DEG C, Dynamic isotherms of hydrogen absorption under 2MPa hydrogen pressure compares, it can be seen that PdMg prepared by said process77Y23Hydrogen bearing alloy compares Mg77Y23Absorption hydrogen ability improves 23%, and hydrogen-absorption speed improves 30% (in the hydrogen-sucking amount 80% that reaches capacity).And subsequently put in hydrogen process, PdMg77Y23Hydrogen bearing alloy hydrogen discharging rate compares Mg77Y23Alloy speeds 42% (to reach hydrogen desorption capacity 80%).
Embodiment 2
Prepare grain graininess 100～120 μm, cladding Pd film thickness 10nm, composition PdMg77Y23Hydrogen bearing alloy
1) dispensing
By purity all metal Mg more than 99.5% and metal Y by design composition Mg77Y23Carry out dispensing, and consider certain scaling loss (scaling loss of Y is set to 5wt%, Mg scaling loss 15wt%)；
2) alloy melting
Fine vacuum high-frequency induction smelting furnace is adopted to prepare Mg-Y foundry alloy.By step 1) raw material for preparing is placed in the graphite crucible of fine vacuum high-frequency induction smelting furnace, is evacuated to background vacuum higher than 5 × 10-4Pa, carries out 3 prepurgings then through with purity >=99.999% argon to furnace chamber, then begins to warm up: first power-on preheated crucible, after 20 seconds, adjusts electric current to 120A, makes alloy block be completely melt；Then improve melting electric current to 240A, keep 2 minutes, after Mg and y alloy fused solution at high temperature mix homogeneously, liquation is poured in copper cold-crucible and condense, obtain certain ingredients as cast condition Mg-Y mother's ingot.
3) break process
By through step 2) the Mg-Y master alloy ingot made carries out Mechanical Crushing and becomes fritter, then be placed in agate mortar and grind to form fine powder, select through 120 mesh sieves, make the alloying pellet that granularity is 100～120 microns.For avoiding granule to aoxidize in atmosphere, break process process completes in glove box.
4) magnetron sputtering Pd film
Choose diameter 60mm, purity >=99.9% Pd target as the negative electrode of magnetron sputtering coater.By through step 3) the kernel alloying pellet made be placed in magnetron sputtering coater sample vibration ware in.Sample vibration ware schematic diagram is as shown in Figure 1.
Arranging sputter coating parameter is: background vacuum 1 × 10-3Pa, adopts purity >=99.99% argon as sputter gas, and argon flow amount is 50sccm, and operating pressure is 0.6Pa, and sputtering power is 150W, and the sputter coating time is 360 seconds.Coating process sample vibration ware frequency of vibration is 5Hz, makes Pd film cladding Mg77Y23Alloying pellet, i.e. PdMg77Y23Hydrogen bearing alloy.
EDAX results shows, PdMg prepared by above-mentioned steps77Y23Hydrogen bearing alloy kernel composition is than for Mg76.9Y23.1, illustrate that female ingot composition is essentially identical with design proportioning；Estimate that Pd film thickness is about 10nm according to inductively coupled plasma atomic emission spectrum (ICP-AES) composition measurement Pd content and in conjunction with granule-morphology, meet designing requirement.
Hydrogen desorption kinetics curve is inhaled it can be seen that the PdMg for preparing of said process from hydrogen bearing alloy77Y23Hydrogen bearing alloy compares Mg77Y23Absorption hydrogen ability improves 27%, and hydrogen-absorption speed improves 33% (in the hydrogen-sucking amount 80% that reaches capacity).And subsequently put in hydrogen process, PdMg77Y23Hydrogen bearing alloy hydrogen discharging rate compares Mg77Y23Alloy speeds 46% (to reach hydrogen desorption capacity 80%).
Embodiment 3
Prepare grain graininess 60～80 μm, cladding Pd film thickness 20nm, composition PdMg77Y23Hydrogen bearing alloy
1) dispensing
By purity all metal Mg more than 99.5% and metal Y by design composition Mg77Y23Carry out dispensing, and consider certain scaling loss (scaling loss of Y is set to 5wt%, Mg scaling loss 15wt%)；
2) alloy melting
Fine vacuum high-frequency induction smelting furnace is adopted to prepare Mg-Y foundry alloy.By step 1) raw material for preparing is placed in the graphite crucible of fine vacuum high-frequency induction smelting furnace, is evacuated to background vacuum higher than 5 × 10-4Pa, carries out 3 prepurgings then through with purity >=99.999% argon to furnace chamber, then begins to warm up: first power-on preheated crucible, after 20 seconds, adjusts electric current to 120A, makes alloy block be completely melt；Then improve melting electric current to 240A, keep 2 minutes, after Mg and y alloy fused solution at high temperature mix homogeneously, liquation is poured in copper cold-crucible and condense, obtain certain ingredients as cast condition Mg-Y mother's ingot.
3) break process
By through step 2) the Mg-Y master alloy ingot made carries out Mechanical Crushing and becomes fritter, then be placed in agate mortar and grind to form fine powder, select through 200 mesh sieves, make the alloying pellet that granularity is 60～80 microns.For avoiding granule to aoxidize in atmosphere, break process process completes in glove box.
4) magnetron sputtering Pd film
Choose diameter 60mm, purity >=99.9% Pd target as the negative electrode of magnetron sputtering coater.By through step 3) the kernel alloying pellet made be placed in magnetron sputtering coater sample vibration ware in.Sample vibration ware schematic diagram is as shown in Figure 1.
Arranging sputter coating parameter is: background vacuum 1 × 10-3Pa, adopts purity >=99.99% argon as sputter gas, and argon flow amount is 50sccm, and operating pressure is 0.6Pa, and sputtering power is 150W, and the sputter coating time is 180 seconds.Coating process sample vibration ware frequency of vibration is 5Hz, makes Pd film cladding Mg77Y23Alloying pellet, i.e. PdMg77Y23Hydrogen bearing alloy.
EDAX results shows, PdMg prepared by above-mentioned steps77Y23Hydrogen bearing alloy kernel composition is than for Mg76.8Y23.2, illustrate that female ingot composition is essentially identical with design proportioning；Observe in conjunction with granule transverse section microscopic appearance, it is known that Pd film thickness is about 20nm, meets designing requirement.
Hydrogen desorption kinetics curve is inhaled it can be seen that the PdMg for preparing of said process from hydrogen bearing alloy77Y23Hydrogen bearing alloy compares Mg77Y23Absorption hydrogen ability improves 31%, and hydrogen-absorption speed improves 35% (in the hydrogen-sucking amount 80% that reaches capacity).And subsequently put in hydrogen process, PdMg77Y23Hydrogen bearing alloy hydrogen discharging rate compares Mg77Y23Alloy speeds 48% (to reach hydrogen desorption capacity 80%).
Embodiment 4
Prepare grain graininess 100～120 μm, cladding Pd film thickness 30nm, composition PdMg77Y23Hydrogen bearing alloy
1) dispensing
By purity all metal Mg more than 99.5% and metal Y by design composition Mg77Y23Carry out dispensing, and consider certain scaling loss (scaling loss of Y is set to 5wt%, Mg scaling loss 15wt%)；
2) alloy melting
Fine vacuum high-frequency induction smelting furnace is adopted to prepare Mg-Y foundry alloy.By step 1) raw material for preparing is placed in the graphite crucible of fine vacuum high-frequency induction smelting furnace, is evacuated to background vacuum higher than 5 × 10-4Pa, carries out 3 prepurgings then through with purity >=99.999% argon to furnace chamber, then begins to warm up: first power-on preheated crucible, after 20 seconds, adjusts electric current to 120A, makes alloy block be completely melt；Then improve melting electric current to 240A, keep 2 minutes, after Mg and y alloy fused solution at high temperature mix homogeneously, liquation is poured in copper cold-crucible and condense, obtain certain ingredients as cast condition Mg-Y mother's ingot.
3) break process
By through step 2) the Mg-Y master alloy ingot made carries out Mechanical Crushing and becomes fritter, then be placed in agate mortar and grind to form fine powder, select through 120 mesh sieves, make the alloying pellet that granularity is 100～120 microns.For avoiding granule to aoxidize in atmosphere, break process process completes in glove box.
4) magnetron sputtering Pd film
Choose diameter 60mm, purity >=99.9% Pd target as the negative electrode of magnetron sputtering coater.By through step 3) the kernel alloying pellet made be placed in magnetron sputtering coater sample vibration ware in.Sample vibration ware schematic diagram is as shown in Figure 1.
Arranging sputter coating parameter is: background vacuum 1 × 10-3Pa, adopts purity >=99.99% argon as sputter gas, and argon flow amount is 50sccm, and operating pressure is 0.6Pa, and sputtering power is 150W, and the sputter coating time is 360 seconds.Coating process sample vibration ware frequency of vibration is 5Hz, makes Pd film cladding Mg77Y23Alloying pellet, i.e. PdMg77Y23Hydrogen bearing alloy.
EDAX results shows, PdMg prepared by above-mentioned steps77Y23Hydrogen bearing alloy kernel composition is than for Mg76.9Y23.1, illustrate that female ingot composition is essentially identical with design proportioning；Estimate that Pd film thickness is about 30nm according to inductively coupled plasma atomic emission spectrum (ICP-AES) composition measurement Pd content and in conjunction with granule-morphology, meet designing requirement.
Hydrogen desorption kinetics curve is inhaled it can be seen that the PdMg for preparing of said process from hydrogen bearing alloy77Y23Hydrogen bearing alloy compares Mg77Y23Absorption hydrogen ability improves 28%, and hydrogen-absorption speed improves 32% (in the hydrogen-sucking amount 80% that reaches capacity).And subsequently put in hydrogen process, PdMg77Y23Hydrogen bearing alloy hydrogen discharging rate compares Mg77Y23Alloy speeds 45% (to reach hydrogen desorption capacity 80%).
Above example is only in order to illustrate that technical scheme is not intended to limit; those of ordinary skill in the field are to be understood that; the specific embodiment of the present invention can being modified with reference to above-described embodiment or equivalent replacement, these are all being applied within the claims awaited the reply without departing from any amendment or equivalent replacement of spirit and scope of the invention.
Claims (8)
1. a high-performance hydrogen bearing alloy PdMg-Y, it is characterised in that interior nuclear composition is Mg100-XYx alloying pellet, x is 20～25, and outer surface is coated with the Pd film of uniform thickness.
2. hydrogen bearing alloy PdMg-Y as claimed in claim 1, it is characterised in that the granularity of kernel Mg-Y is 50～150 microns.
3. hydrogen bearing alloy PdMg-Y as claimed in claim 1, it is characterised in that Pd film thickness is 5～30nm.
4. the preparation method of hydrogen bearing alloy PdMg-Y as described in any one of claims 1 to 3, comprises the steps of:
A, dispensing: metal Mg and metal Y is according to the ratio dispensing that mol ratio is 3:1～4:1；
B, prepare foundry alloy: be placed in the graphite crucible of smelting furnace by raw material, evacuation, purges 3～5 times furnace chamber with argon, then heats the Mg being uniformly mixed and y alloy fused solution, described melting charge is poured in copper cold-crucible and condense, obtain as cast condition Mg-Y master alloy ingot；
C, the Mg-Y master alloy ingot made by step b are pulverized, and cross 100～300 mesh sieve choosings, make the alloying pellet that granularity is 50～150 microns；
D, the negative electrode being magnetron sputtering coater with Pd target, be placed on the alloying pellet that step c prepares in the sample vibration ware of magnetron sputtering coater, be coated with Pd film, obtain hydrogen bearing alloy PdMg-Y.
5. the preparation method of PdMg-Y hydrogen bearing alloy as claimed in claim 4, it is characterised in that the purity of metal Mg and metal Y is all more than 99.5%.
6. the preparation method of PdMg-Y hydrogen bearing alloy as claimed in claim 4, it is characterised in that the vacuum of described b step is higher than 5 × 10-4Pa；Purity of argon >=99.999% of purging furnace chamber；After preheating 20～30 seconds, electric current is adjusted to 120～160A, after making the fusing of alloy block, electric current is risen to 200～350A again, heat 2～3 minutes.
7. the preparation method of PdMg-Y hydrogen bearing alloy as claimed in claim 4, it is characterised in that step c completes in vacuum glove box.
8. the preparation method of PdMg-Y hydrogen bearing alloy as claimed in claim 4, it is characterised in that the target diameter of negative electrode Pd described in step d is 60～80mm, purity >=99.9%；Background vacuum 1 × 10-3～2 × 10-3Pa, with purity >=99.99% sputtering argon, is 40～80sccm in argon flow amount, and pressure is under 0.5～0.8Pa, and sputtering power is under 120～200W, sputters 120～300 seconds；Sample vibration ware frequency of vibration is 5～20Hz.
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| CN108615850A (en) * | 2018-04-20 | 2018-10-02 | 北京大学 | A kind of Combined electrode and its preparation for air cell |
| CN109234695A (en) * | 2018-11-15 | 2019-01-18 | 杭州电子科技大学 | A kind of preparation method of nanocrystalline intermetallics hydrogen storage material |
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| CN108584870B (en) * | 2018-07-18 | 2020-08-18 | 江苏兴贤高新材料股份有限公司 | Preparation method of environment-friendly hydrogen storage material |
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| CN103668133A (en) * | 2013-09-09 | 2014-03-26 | 西北工业大学 | Method for Zr-based hydrogen storage alloy deposition of Pd film and plating solution for chemical plating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108615850A (en) * | 2018-04-20 | 2018-10-02 | 北京大学 | A kind of Combined electrode and its preparation for air cell |
| CN108615850B (en) * | 2018-04-20 | 2021-06-01 | 北京大学 | Composite electrode for air battery and preparation method thereof |
| CN109234695A (en) * | 2018-11-15 | 2019-01-18 | 杭州电子科技大学 | A kind of preparation method of nanocrystalline intermetallics hydrogen storage material |
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